HRID2229994

反应详情

EQUATION

反应方程式

HRID 2229994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In this step, synthesis of an active ester of a binding enhancer is described, which can then be easily conjugated to both the photoreactive ligand and the linker. A solution of bisbenzimidazole (6 g, 0.01 mol) dicyclohexylcarbodiimide (0.05 mol) and succinic acid (0.01 mol) in 100 mL of chloroform is stirred overnight ( 18-24 hrs). During this time, a white precipitate is formed. The precipitate is filtered of and washed with chloroform (2×50 mL). The combined chloroform is concentrated under vacuum in a rotary evaporator and the residue purified by flash column chromatography. The fractions containing the product is combined and concentrated under vacuum in a rotary evaporate to afford bisbenzimide succinnate ester (80%) as a white solid.

WORKUP

后处理

  1. customDuring this time, a white precipitate is formed
  2. filtrationThe precipitate is filtered of and
  3. washwashed with chloroform (2×50 mL)
  4. concentrationThe combined chloroform is concentrated under vacuum in a rotary evaporator
  5. customthe residue purified by flash column chromatography
  6. additionThe fractions containing the product
  7. concentrationconcentrated under vacuum in
  8. customa rotary evaporate